Treatment of waxes



Patented Nov. 26, 1935 UNITED STATES iATENT OFFICE TREATMENT (PF WAXESNo Drawing. Application March 16, 1933, Serial No. 661,176. In GreatBritain March 1'7, 1932 4 Claims.

True fats and fatty oils consist essentially of glyoerides of higherfatty acids and, as is well known are easily saponified to give soapsand glycerine. Waxes also consist of or contain esters of fatty acids,but these esters are not glycerides; they are the esters of highermonohydric alcohols. When the distinction between fats and Waxes is thusdrawn on a chemical basis, there come to be classed among the waxes thethe so-called liquid waxes, sperm oil and arctic sperm oil.

The present invention relates to a treatment of waxes, liquid or solid,whereby the esters present are saponified and the alcohols are separatedin a technically advantageous way.

Known methods of saponifying waxes are not adapted to be performed on amanufacturing scale. When aqueous alkali is used much troublesome-frothis formed and it is difficult to separate the alcohol from the soap. Tosaponify with alcoholic alkali is too costly. It has been proposed toseparate alcoholic material, adapted for pharmaceutical use, fromspermaceti by a treatment with lime, followed by distillation (Axelrad,Journal of Industrial and Engineering Chemistry, 1917, 9, 1123) but thisprocess is not free from technical disadvantages because the lime, limesoaps, etc. of which the mass to be distilled consists do not melt.

According to the present invention we heat together a liquid or solidwax and either dry caustic potash or a dry mixture of caustic potash andcaustic soda and separate the alcohol from the molten reaction mass by adistillation process.

When a wax and dry caustic potash or a dry mixture of caustic potash andcaustic soda are heated together in accordance with the invention amixture of fatty alcohol and anhydrous soap is formed. This is molten ata temperature such that the alcohol can be separated by distillation.

The distillation is preferably carried out by use of superheated steam,and it can then be carried out usually at atmospheric pressure.Distillation may also be effected under diminished pressure, with orwithout simultaneous use of steam.

In using superheated steam it is not necessary that the steam should besuperheated before it is admitted to the distillation vessel, itsuffices that dry steam such as is commonly available in factoryprocesses, be passed into the vessel, the contents of which are kept atthe desired temperature by appropriate external heating.

Distillation proceeds smoothly because the material in the still isliquid. So that distillation may take place at the lowest convenienttemperature it is advantageous to use not caustic potash alone, but amixture of caustic potash and caustic soda, the proportions of causticpotash and caustic soda being so chosen that preferably the soapremaining at the end of the distillation is a eutectic mixture.

The invention is illustrated but not limited by the following examples,the parts are by weight.

Example 1 241 parts of spermaceti are melted and heated to 200 C. 42parts of powdered potassium hydroxide are now added with agitation inhalf an hour, during which time the temperature is allowed torise to 240C. It is held at this temperature for half an hour when superheatedsteam is passed in. There distils over with the steam a colourless oilwhich sets on cooling to a crystalline waxy solid which is entirely freefrom fatty acid and from unsaponified spermaceti. The yield isapproximately parts by weight, the proportion of water to oil in thedistillate being approximately 10:1.

Example 2 241 parts of spermaceti are treated as in Example l with amixture of 21 parts powdered potassium hydroxide and 15 parts ofpowdered sodium hydroxide. After reaction, the molten mixture of soapsand fatty alcohol is subjected to superheated steam distillation atabout 250 C., eventually at 280 C. until no more oil distils. The yieldis approximately 100 parts of the pure alcohol from spermaceti, theratio of water to oil in the distillate being approximately 10:1.

Example 3 268 parts of sperm oil are treated as in Example 1 with amixture of 21 parts of caustic potash and 15 parts of caustic soda.After reaction the mass is subjected to superheated steam distillationuntil no more oil distils. The yield is 90 parts of a semi-solidalcohol, free from unsaponified wax or free fatty acid. The ratio ofwater to oil in the distillate is approximately 4:1.

Example 4 290 parts of beeswax are heated to C. 50 and a mixture of 16parts of powdered caustic potash and 11% parts of powdered caustic sodais added. The mixture is then treated with superheated steam asdescribed in the preceding examples. Myricyl alcohol is obtained, theratio 55 of water to alcohol in the distillate being about 25:1.

Other waxes, e. g. chinese wax, wool fat, carnauba wax may be treated inthe same way.

We claim:

1, Process for the manufacture of higher alcohols comprising heating awax with a dry mixture of caustic potash and caustic soda in proportionssuch as to give a eutectic mixture of the corresponding soaps.

2. Process for the manufacture of higher alcohols comprising heating aWax with a dry mixture of caustic potash and caustic soda in proportionssuch as to give a eutectic mixture of the corresponding soaps andseparating the alcohol by distillation.

3. Process for the manufacture of an alcohol from spermaceti wax whichcomprises heating substantially 241 parts of the Wax with a mixture ofabout 21 parts of dry caustic potash and about 15 parts of dry causticsoda at about 200-240 (3., and thereafter distilling oi? the alcohol ina current of superheated steam.

4. Process for the manufacture of an alcohol from sperm oil whichcomprises heating substantially 268 parts of the liquid war; with amixture of about 21 parts of dry caustic potash and about 15 parts ofdry caustic soda at about ZOO-240 C., and thereafter distilling oil thealcohol in a current of superheated steam.

WILFRED ARCHIBALD SEXTON. DENIS WARD.

